RESUMO
Reference materials for quantitative determination of Cd, Cr, Hg and Pb in polycarbonate were developed. Reference materials with two concentration level of elements were prepared by adding appropriate amounts of chemicals to a blank polycarbonate base material. It was shown that ten bottles with triplicate analysis are enough to demonstrate the homogeneity of these candidate reference materials. The statistical results also showed no significant trends in both short-term stability test for four weeks and long-term stability test for twelve months. The certification of the four elements was carried out by isotope-dilution-inductively coupled plasma mass spectrometry (ID-ICP-MS) with microwave-assisted digestion. Certification of candidate reference materials in a single laboratory was confirmed with interlaboratory comparison participated by a certain number of well-recognized testing laboratories in Korea. The certified values and expanded uncertainties (k=2) for the candidate reference material with low level and the one with high level were (51.7±2.1)mgkg(-1) Cd, (103.8±2.9)mgkg(-1) Cd, (98.8±4.5)mgkg(-1) Cr, (1004±49.8)mgkg(-1) Cr, (107.4±4.6)mgkg(-1) Hg, (1133±50.7)mgkg(-1) Hg, (94.8±3.7)mgkg(-1) Pb and (988.4±53.6)mgkg(-1) Pb, respectively. The reference materials developed in this study demonstrated their suitability for the quality assurance in Cd, Cr, Hg and Pb analysis for the implementation of RoHS Directive.
RESUMO
An organic-assisted alkaline extraction method was developed for the determination of hexavalent chromium (Cr(VI)) in plastics. The solubilization of polymer as a pre-step of the alkaline extraction provided good extraction efficiency of Cr(VI) from the sample. The optimization of the experimental conditions affecting the extraction and UV-vis spectrophotometric analysis was accomplished by evaluating the recovery rate of Cr(VI) through the analysis of Cr(VI) in in-house polymer reference materials (RMs). With the proposed method, most of the Cr(VI) in polymers was released within a short extraction time of 30 min and the Cr(III)-DPCO complex can be kept stable for 24 h. The heating for the extraction of the Cr(VI) was not necessary. The optimal pH of the final solution was fixed at 2.0. The proposed extraction method was applied successfully for the determination of Cr(III) and Cr(VI) in spiked samples. The practical applicability of this new method was evaluated through the analysis of Cr(VI) in in-house polymer RMs. The good linearity was demonstrated at desired concentrations of the range 0-3.3 mg L(-1). The detection limits were quite low, varying from 0.0061 to 0.0285 mg L(-1). The recovery of Cr(VI) was between 97 and 106%, and the relative standard deviation (R.S.D.) was below 6%.
RESUMO
We have developed a method to fabricate graphene flakes composed of high quality multi-layer graphene sheets using a thermal plasma jet system. A carbon atomic beam was generated by injecting ethanol into Ar plasma continuously; the beam then flowed through a carbon tube attached to the anode. Graphene was made by epitaxial growth where a carbon atomic beam, having the proper energy, collided with a graphite plate. The graphene fabricated was very pure and showed a relatively good crystalline structure. We have demonstrated that the number of layers of graphene sheets could be controlled by controlling the rate of ethanol injection. Our process is a continuous process with a relatively high yield (approximately 8%).